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Chromatographic and Mass Spectral Analyses of Oligosaccharides and Indigo Dye Extracted from Cotton Textiles with Manova and Ano

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Chromatographic and Mass Spectral Analyses of Oligosaccharides and Indigo Dye Extracted from Cotton Textiles with Manova and Ano University of Central Florida STARS Electronic Theses and Dissertations, 2004-2019 2008 Chromatographic And Mass Spectral Analyses Of Oligosaccharides And Indigo Dye Extracted From Cotton Textiles With Manova And Ano Jessica Frisch University of Central Florida Part of the Chemistry Commons, and the Forensic Science and Technology Commons Find similar works at: https://stars.library.ucf.edu/etd University of Central Florida Libraries http://library.ucf.edu This Masters Thesis (Open Access) is brought to you for free and open access by STARS. It has been accepted for inclusion in Electronic Theses and Dissertations, 2004-2019 by an authorized administrator of STARS. For more information, please contact [email protected]. STARS Citation Frisch, Jessica, "Chromatographic And Mass Spectral Analyses Of Oligosaccharides And Indigo Dye Extracted From Cotton Textiles With Manova And Ano" (2008). Electronic Theses and Dissertations, 2004-2019. 3625. https://stars.library.ucf.edu/etd/3625 CHROMATOGRAPHIC AND MASS SPECTRAL ANALYSES OF OLIGOSACCHARIDES AND INDIGO DYE EXTRACTED FROM COTTON TEXTILES WITH MANOVA AND ANOVA STATISTICAL DATA ANALYSES by JESSICA LYNNE FRISCH B.S. University of Central Florida, 2005 A thesis submitted in partial fulfillment of the requirements for the degree of Master of Science in the Department of Chemistry in the College of Sciences at the University of Central Florida Orlando, Florida Spring Term 2008 © 2008 Jessica Lynne Frisch ii ABSTRACT Research was conducted on thirteen 100% cotton denim samples using an acid wash, established by Murray, to extract oligosaccharides from the cellulosic material. The oligosaccharide ion + + + groups ([M+H] , [M+NH4] , and [M-OH] ) for molecules with degrees of polymerization between two and seven (DP2-DP7) were analyzed using liquid chromatography coupled to mass spectrometry with an electrospray ionization interface (LC-ESI-MS). The results were compared using the least-squares means in a Multivariate ANOVA (MANOVA) test followed by Univariate ANOVA and Tukey HSD tests and demonstrated that the method could correctly determine that two samples were statistically different 85.9% of the time when analyzing the amount (ng) of each of the oligosaccharide ion groups separately, and 82.0% when analyzing the total moles of monosaccharide units released. A dye extraction was performed on the denim materials and the extract analyzed using gas chromatography coupled with mass spectrometry (GC-MS). Indigo dye was present in all of the denim samples except one. When these results were combined with the two oligosaccharide statistical analyses, the discriminating power was increased to 88.5% and 85.9%, respectively. Additional cellulosic materials were also investigated including four white 100% cotton t-shirts as well as five raw cotton samples grown in Tajikistan, Uzbekistan, Egypt, Iran, and Benin West Africa. The analytical methodology gave results for the white cotton t-shirts and raw cotton samples that were inconsistent with those obtained from the denim samples. iii This thesis is dedicated to the memory of my Dad. David Mark Frisch May 23, 1957 – September 2, 2005 He will always be loved and shall forever live on in my heart. iv ACKNOWLEDGMENTS I would like to express my sincere gratitude to: my mom, Cheryl Frisch – for her prayers; Uncle Bill and Aunt Nora – for always being there for me; my step-mom, Kathy – for supporting me and my education; my youngest sister, Clara, and my brother, Robert – for always making me smile and inspiring me to be the kind of individual they can look up to; my supportive friends Alisha and Bryan Yabczanka, Clare Kidwell, Nathan Costa, Kyle and Erin Parker, LeAnn and Ryan Lett, Diane Kodera, and my boyfriend Chris Daiello – for their continuous encouragement and friendship; my co-workers past and present at NCFS, Mary Williams and Katie Steele –for demonstrating how to successfully defend a thesis; Doug Clark – for putting up with questions, despite how ridiculous; “Miss Judy” Stout – if it was not for her chocolate candy stash, I do not know how I would have made it through all the “Mondays”; April Marrone – for her trouble- shooting help with the instrument and for making 242 my new “favorite” number; my co-worker, roommate and friend, Erin McIntee – for her help with what seemed like endless sample extractions and having the patience to hear me talk about my research/thesis endlessly; Dr. Candice Bridge – for inspiring me to go for my Ph.D. I would like to thank Dr. Fookes and Dr. Hampton for serving on my thesis committee and helping me when I needed it, and Dr. Ni for all of his help with statistics. Finally, I would especially like to thank Dr. Sigman for all of his help, support, and for challenging me. I could not have asked for a better adviser. “A mind, once stretched by a new idea, never returns to its original dimensions." Oliver Wendell Holmes v TABLE OF CONTENTS LIST OF FIGURES ....................................................................................................................... ix LIST OF TABLES......................................................................................................................... xi CHAPTER 1: INTRODUCTION................................................................................................... 1 CHAPTER 2: BACKGROUND INFORMATION AND LITERATURE REVIEW .................... 4 2.1 Cotton.................................................................................................................................... 4 2.1.1 Cotton Introduction........................................................................................................ 4 2.1.2 Cotton Structure............................................................................................................. 7 2.1.3 Classifying and Manufacturing Cotton for Textiles .................................................... 13 2.1.4 Cotton Fiber Frequency and Discrimination................................................................ 21 2.2 Oligosaccharide Analyses and Differentiation of Cellulosic Materials.............................. 25 2.2.1 Work by Allen K. Murray............................................................................................ 26 2.2.2 Additional Methods of Analyses ................................................................................. 30 2.3 Instrumentation ................................................................................................................... 38 2.3.1 LC-ESI-MS.................................................................................................................. 38 2.3.2 GC-MS......................................................................................................................... 54 2.4 Statistical Methods of Analyses.......................................................................................... 57 2.4.1 One-way Analysis of Variance .................................................................................... 57 2.4.2 Multivariate Analysis of Variance............................................................................... 61 CHAPTER 3: OLIGOSACCHARIDE ANALYSIS .................................................................... 64 3.1 Instrument Parameters ........................................................................................................ 64 3.2 Oligosaccharide Extraction and Isolation from Cellulosic Material................................... 68 vi 3.2.1 Oligosaccharide Acid Extraction ................................................................................. 69 3.2.2 Isolation of Oligosaccharides....................................................................................... 69 3.3 Standards............................................................................................................................. 71 3.3.1 Sample Collection and Preparation.............................................................................. 71 3.3.2 Analyses and Results ................................................................................................... 71 3.4 Denim.................................................................................................................................. 78 3.4.1 Sample Collection and Preparation.............................................................................. 78 3.4.2 Analyses and Results ................................................................................................... 81 3.5 White Cotton T-Shirts......................................................................................................... 99 3.5.1 Sample Collection and Preparation.............................................................................. 99 3.5.2 Analyses and Results ................................................................................................. 100 3.6 Raw Cotton ....................................................................................................................... 103 3.6.1 Sample Collection and Preparation............................................................................ 103 3.6.2 Analyses and Results ................................................................................................. 104 CHAPTER 4: DYE ANALYSIS ................................................................................................ 107 4.1 Instrumentation Parameters .............................................................................................
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